title: Pre-study and in-study validation of a SPE-LC-MS-MS method for the determination of 5-S-cysteinyldopa, a melanoma biomarker, in human plasma.
abstract: The incidence of malignant melanoma has increased over the past decades, particularly in Caucasian population. This disease presents defavourable prognosis in terms of survey, especially when detection occurs at the metastatic phase. Reliable analytical methods for biomarker determination are thus an interesting tool in pathology detection and follow-up. In this context, a method using SPE-LC-ESI-MS-MS for the determination of 5-S-cysteinyldopa (5-SCD) in human plasma was optimized. The presence of matrix effect was investigated in details while 5-SCD stability was studied according to FDA requirements for the validation of bioanalytical methods. Pre-study and in-study validations of the entire method were then successfully performed by applying the approach based on total measurement error and accuracy profiles over a concentration ranges from 1.6 to 200 ng/ml. Good results with respect to accuracy, trueness and precision were obtained. The maximum risk of observing future measurements falling outside the acceptance limits during routine analysis was also estimated.
authors.affiliation: Laboratory of Analytical Pharmaceutical Chemistry and Bioanalysis, Department of Pharmacy, CIRM, University of Liège, CHU, B36, B-4000 Liège, Belgium.
authors.forename: Gaëlle
authors.initials: G
authors.lastname: Martin
authors.forename: François
authors.initials: F
authors.lastname: Mansion
authors.forename: Virginie
authors.initials: V
authors.lastname: Houbart
authors.forename: Philippe
authors.initials: P
authors.lastname: Paquet
authors.forename: Andrée
authors.initials: A
authors.lastname: Rorive
authors.forename: Patrice
authors.initials: P
authors.lastname: Chiap
authors.forename: Jacques
authors.initials: J
authors.lastname: Crommen
authors.forename: Anne-Catherine
authors.initials: AC
authors.lastname: Servais
authors.forename: Marianne
authors.initials: M
authors.lastname: Fillet
mesh_terms: D014408:Biomarkers, Tumor / Q000097:blood*; D002138:Calibration; D002853:Chromatography, Liquid / Q000379:methods*; D003548:Cysteinyldopa / Q000097:blood*; D006801:Humans; D057230:Limit of Detection; D008545:Melanoma / Q000097:blood*; D012015:Reference Standards; D015203:Reproducibility of Results; D052616:Solid Phase Extraction / Q000379:methods*; D053719:Tandem Mass Spectrometry / Q000379:methods*
chemical_list: D014408:Biomarkers, Tumor; D003548:Cysteinyldopa